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ORA LABORATORY PROCEDURE Document No.: Version No.: 1.

3
Food and Drug Administration ORA-LAB. 5.6
Page 1 of 7
Title: Effective Date:
MEASUREMENT TRACEABILITY 10-01-03
Revised: 11/16/06

Sections Included in this Document and Document History


1. Purpose
2. Scope
3. Responsibilities
4. Background
5. References
6. Procedure/(Changed two years to annually in 6. C. 2.)
7. Definitions
8. Records
9. Supporting Documents
10. Attachments
Document History

1. This procedure describes how the laboratory achieves measurement


Purpose traceability for its measuring and testing equipment, as well as for its physical
standards and media.

2. This procedure addresses the traceability of Office of Regulatory Affairs


Scope (ORA) Laboratory instruments used for measuring and testing. It also
addresses equipment used for the direct measurement of fundamental
properties, such as balance masses and thermometers.

3. ORA laboratories are responsible for maintaining records of measurement


Responsibilities traceability. These records include certificates for the calibration of the
balance masses and. Thermometers. They also include the certificates for
reference materials used to calibrate or standardize laboratory equipment and
for reference cultures.

4.
Background None

5. ISO/IEC 17025. General requirements for the competence


References of testing and calibration laboratories (5.6 Measurement
Traceability). Geneva, Switzerland: The International Organization for
Standardization and the International Electrotechnical Commission.

Taylor, J. K. (1993). Handbook for SRM users (NBS Special Publication No.
260-100). Gaithersburg, MD: National Institute for Standards and
Technology.

_____________________________________________________________________________________________

This document is uncontrolled when printed: 8/11/2008


For the most current and official copy, check the Internet at
http://www.fda.gov/ora/science_ref/lm/default.htm
ORA LABORATORY PROCEDURE Document No.: Version No.: 1.3
Food and Drug Administration ORA-LAB. 5.6
Page 2 of 7
Title: Effective Date:
MEASUREMENT TRACEABILITY 10-01-03
Revised: 11/16/06

6. A. Measurement Traceability
Procedure
1. Reference balance masses, thermometers and thermocouples are
traceable to international standard (SI) units of measurement.

2. Laboratory measuring equipment is calibrated or standardized using


materials of known and acceptable purity (i.e. neat compounds, or
reference materials of know composition traceable to national,
international or equivalent standards).

3. Media are verified against national or international standards (i.e.


reference cultures or certified reference cultures).

4. The traceability to SI units is achieved by reference to national


measurement standards that are primary realizations of the SI units or
agreed representations of SI units. SI units are based on fundamental
physical constants of mass, distance, and time.

5. Traceability may also be established through secondary standards that


are calibrated by a national metrology institute such as the National
Institute for Standards and Technology (NIST).

B. Traceability Alternatives to SI Units

1. Where calibrations cannot provide measurement traceability to SI


units, confidence in measurements is established with traceability to
measurement standards such as:

• certified reference materials provided by a competent supplier to


give a reliable physical or chemical characterization of a material,
and

• the use of specified methods and consensus standards that are


clearly described and agreed by the parties concerned.

2. Where traceability of measurements to SI units is not possible or not


needed, the same requirements for traceability, for example, certified
reference materials, agreed methods or consensus standards, are
needed.

3. For some analyses certified reference materials are not readily found.
In this case, a material with similar properties and stability is selected.
_____________________________________________________________________________________________

This document is uncontrolled when printed: 8/11/2008


For the most current and official copy, check the Internet at
http://www.fda.gov/ora/science_ref/lm/default.htm
ORA LABORATORY PROCEDURE Document No.: Version No.: 1.3
Food and Drug Administration ORA-LAB. 5.6
Page 3 of 7
Title: Effective Date:
MEASUREMENT TRACEABILITY 10-01-03
Revised: 11/16/06

The properties of interest in this material is characterized by repeat


testing, preferably by more than one laboratory and using a variety of
methods.

4. Where national or international standards are not found for the


verification of the performance of microbiology procedures, the
laboratory documents recovery by either participating in a program of
interlaboratory comparison or proficiency testing, use of reference
cultures or certified reference cultures, or by a mutual agreement with
client on expectations.

C. Calibration and Calibration Services for Physical Standards

1. Calibration is conducted for the physical standards used by the


laboratory by an accredited calibration laboratory who provide the
laboratory with certificates of calibration linking the calibrations to
measurements made by NIST or some equivalent. The identity of the
calibration laboratory is included on the certificate as well as the
methods and standards primary to the process.

2. Traceable thermometers are calibrated annually, thermocouples every


year, and masses are calibrated every five years. These reference
standards are used for calibration checks only and not as working
standards.

3. A calibration certificate bearing an accreditation body logo from a


calibration laboratory accredited to the International Organization for
Standardization and the International Electrotechnical Commission
(ISO/IEC) 17025 standard for the calibration concerned is sufficient
evidence of traceability of the calibration data reported.

4. The date of calibration and the date of the next calibration that is due
is included for the reference standard in the calibration certificates.

5. These reference standards are stored in a secured area to prevent any


damage that would invalidate their use.

6. Servicing is requested from the calibration laboratory when data


acceptance criteria for verification are not met and the analyst is
unable to effect a corrective action.

D. Calibration of Laboratory Measuring Instruments


_____________________________________________________________________________________________

This document is uncontrolled when printed: 8/11/2008


For the most current and official copy, check the Internet at
http://www.fda.gov/ora/science_ref/lm/default.htm
ORA LABORATORY PROCEDURE Document No.: Version No.: 1.3
Food and Drug Administration ORA-LAB. 5.6
Page 4 of 7
Title: Effective Date:
MEASUREMENT TRACEABILITY 10-01-03
Revised: 11/16/06

1. Calibration or standardization of laboratory instruments is conducted


according to the test method employed. The uncertainty contributions
are addressed in ORA Laboratory Manual, Volume II, Section 2,
ORA-LAB.5.4.6. Estimation of Uncertainty of Measurement.

2. Instruments identified in the test methods which call for calibrations as


part of their normal operation are calibrated by laboratory personnel
who conduct these operations using reference materials.

3. Reference materials, where possible, are to be traceable to SI units of


measurement, to standard reference materials (SRMs), certified
reference materials (CRMs), or certified reference cultures (CRCs).

4. Certificates of Analysis from the manufacturer for reference materials


used are maintained.

5. A listing of reference materials in use in the laboratory is maintained.


This listing will contain, as a minimum, the chemical name or
description, source, manufacturer’s lot number, laboratory number (if
lot number not used), date of receipt, and expiration date, if present.

6. Reference materials are labeled with date of receipt and initials, date
opened and initials, and expiration date.

7. Analyst’s records include the identity of and the measurement values


for standards or reference materials used in the routine analyses. This
information is to have record traceability to the measurements for
batches of samples measured sequentially to the standard or reference
material. This information is recorded in the analytical worksheets,
instrument logbooks or incorporated in the instrument print out for the
analyses.

8. Calibration is verified during the performance of analyses. The


frequency of calibration is identified in the test method or per
laboratory instrument procedure.

9. The safe handling, transport, storage, and use of laboratory reference


materials are conducted according to the manufacturer’s instructions in
order to prevent contamination, deterioration, and to protect their
integrity.

_____________________________________________________________________________________________

This document is uncontrolled when printed: 8/11/2008


For the most current and official copy, check the Internet at
http://www.fda.gov/ora/science_ref/lm/default.htm
ORA LABORATORY PROCEDURE Document No.: Version No.: 1.3
Food and Drug Administration ORA-LAB. 5.6
Page 5 of 7
Title: Effective Date:
MEASUREMENT TRACEABILITY 10-01-03
Revised: 11/16/06

10. Reference materials are not stored with samples.

E. Reagents, solvents, gases, and media

1. For most analyses, analytical reagent grade is satisfactory. Trace


analyses frequently call for special ultra pure reagents, solvent and
gases.

2. Reagent grade chemicals should be ordered in quantities such that the


supply will be consumed within the manufacturer’s expiration date or
five years, whichever is first.

3. All reagents, solutions and media are labeled with date of receipt and
initials, date opened and initials, and expiration date.

4. Reagents, solvents, gases, and media are stored according to the


manufacturer’s direction and are not be kept longer than recommended
by the manufacturer or the method. Reagents are checked for signs of
deterioration. Reagents that have deteriorated are not used and are
discarded in accordance with a Laboratory’s Safety and Hazardous
Waste procedures.

5. Media purchased or prepared are evaluated for suitability.

F. Disposal

Reference materials, reagents, solvents, gases, and media are disposed of


according to federal, state and local regulations. The laboratory has
procedures for the proper disposal.

7. Calibration – A calibration is the set of operations which establish, under


Definitions specified conditions, the relationship between values indicated by a
measuring instrument or measuring system, or values represented by a
material measure, and the corresponding known values of a known values of
a measurand.

Calibration laboratory - a calibration laboratory provides calibration services


as its principal activity. This type of laboratory is also referenced as a
metrology laboratory.

Certified reference cultures (CRC) – These are cultures traceable to

_____________________________________________________________________________________________

This document is uncontrolled when printed: 8/11/2008


For the most current and official copy, check the Internet at
http://www.fda.gov/ora/science_ref/lm/default.htm
ORA LABORATORY PROCEDURE Document No.: Version No.: 1.3
Food and Drug Administration ORA-LAB. 5.6
Page 6 of 7
Title: Effective Date:
MEASUREMENT TRACEABILITY 10-01-03
Revised: 11/16/06

nationally or internationally recognized type culture collection (i.e. American


Type Culture Collection).

Certified reference material (CRM) – A certified reference material is one or


more of whose property values are certified by a technical valid procedure,
accompanied by or traceable to a certificate or other documentation which is
issued by a certifying body.

International standard – These are standards from an international repository


that fulfill the properties of primary standards for the realization of SI units.
Measurand – A measurand is a particular quantity subject to measurement.

Measuring and testing equipment – These are devices used by the laboratory
for testing and measurement. Equipment, instruments, and instrumentation
are terms used synonymously with measuring and testing equipment.

National Standard – These standards are from a national repository that


fulfill the properties of primary standards for the realization of SI units.

Reference material (RM) - A reference material is one or more of whose


property values are sufficiently well established to be used for calibration or
standardization of an apparatus, the assessment of a measurement method, or
for assigned values to materials.

Reference standard – This is a standard generally of the highest metrological


quality found at a given location, from which measurements made at that
location are derived.

Standard reference material (SRM) - a certified reference material produced


by the National Institute for Standards and Technology or a certified
reference material whose metrological values are approved by a nationally
recognized measurement body. The National Institute for Standards and
Technology is the United States nationally recognized measurement body.

Standardization – This is the assignment of a compositional value to one


standard (measurand) based upon another standard.

Traceability – Traceability is an unbroken chain of calibrations or


comparisons to identified primary standards of the SI units of measurement.

Verification – Verification is confirmation by examination and provision of


evidence that specified requirements have been met.
_____________________________________________________________________________________________

This document is uncontrolled when printed: 8/11/2008


For the most current and official copy, check the Internet at
http://www.fda.gov/ora/science_ref/lm/default.htm
ORA LABORATORY PROCEDURE Document No.: Version No.: 1.3
Food and Drug Administration ORA-LAB. 5.6
Page 7 of 7
Title: Effective Date:
MEASUREMENT TRACEABILITY 10-01-03
Revised: 11/16/06

8. List of standards used by the laboratory


Records Reference materials certificates
Physical standards certificates of traceability
Media suitability records

9. ORA lab manual of quality policies and procedure, Volume II, Section 2
Supporting ORA-LAB.5.5 Equipment
Documents Laboratory Hazardous Waste Management Plan
Laboratory Chemical Management Plan
Microbiology Laboratory media procedure for preparation, labeling and
quality control
10.
Attachments None

Document History
Version Status Date Location of Name & Title
No. (I, R, C) Approved Change History Author Approving Official
1.2 R 11/16/05 In Document LMEB LMEB
1.3 R 12/06/06 In Document LMEB LMEB

Approving Official’s signature: ___________________________________ Date: ____________

_____________________________________________________________________________________________

This document is uncontrolled when printed: 8/11/2008


For the most current and official copy, check the Internet at
http://www.fda.gov/ora/science_ref/lm/default.htm